气相色谱-质谱联用法测定维生素C泡腾片中的甜蜜素

采用气相色谱-质谱(GC-MS)选择离子监测法(SIM),建立了准确可靠、灵敏度高、快速简便的测定维生素C泡腾片中甜蜜素含量的新方法.样品中的甜蜜素衍生后用有机试剂提取,在选择离子模式下进行测定,以保留时间和特征离子比例进行定性,单离子定量.甜蜜素的线性范围为0.05-10mg/L,检出限为0.6mg/kg,回收率为90.5%-96.9%,相对标准偏差小于4.4%.方法分析所用时间短,结果准确可靠,选择性好,适用于维生素C泡腾片中甜蜜素含量的检验.     

Optimization of a Cryogenic System at Temperature 2 K for the PKU-FEL Facility

The conceptual design of a cryogenic system at temperature 2 K for the Peking University Free Electron Laser （PKU-FEL） facility is carried out. In order to minimize the scale of the cryogenic system and the running cost, the superconducting accelerator and the superconducting injector will mainly run at a long-pulsed mode. Optimization of the 2-K cryogenic system is carried out based on the heat load estimation and running parameters. Total cooling power of 52.5 W for the long-pulsed mode is necessary for the PKU cryogenic system. The PKU cryogenic system will be the first 2-K system for accelerators in China and will provide experience for similar facilities.     

Crystal structure and morphology of phenyl‐capped tetraaniline in the leucoemeraldine oxidation state

A series of crystals of phenyl‐capped tetraaniline in the leucoemeraldine oxidation state were obtained at different isothermal temperatures and were observed directly under transmission electron microscope. The crystals obtained at higher temperatures exhibit more perfect structures than those obtained at lower temperatures. Both the lamella thickness and the crystal size increase with crystallization temperature. The tetraaniline is apt to form larger scale crystals under lower degree of supercooling. However, their crystal structures keep steady with the crystallization temperature. The tetramer was found to adopt a monoclinic lattice with unit cell parameter of a = 13.93 Å, b = 8.82 Å, c = 23.20 Å, and β = 95.03°, as determined using electron diffraction tilting method combined with wide‐angle X‐ray diffraction experiment. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 764–769, 2006     

一种高效驱蚊剂的合成

一种高效驱蚊剂的合成高明章（西江大学轻工化学系肇庆５２６０６１）关键词驱蚊剂ＤＥＴＡ合成中图分类号Ｏ６２５．５为了驱避蚊虫，人们进行了多年的研究，合成了许多驱蚊剂，到１９７５年止，各国合成和试验过的化合物就有２５００种以上［１］。其中Ｎ，Ｎ－二乙基间...     

反对数微分简易示波伏安法的研究

在获得微分简易地波伏安图的实验线路中,增加了反对数装置,提出了反对数微分简易示波伏安法。该方法被应用于铝合金中微量铜和分子筛中微量钴的测定,获得了满意结果。     

电子探针定量分析的标准样品——几种多元氧化物单晶

在很高的温度和适宜的生长条件下,分别采用熔盐籽晶法和高温引上法生长了高质量的YAP、NAB、KTP、LN、BBO、SBN等多元氧化物单晶,它们具有优良的物理化学性能,严格的化学比,固定的组成与结构以及较好的化学均匀性和电子束轰击下的稳定性。广泛地用于激光和非线性光学领域。我们选用这些晶体为原材料研制电子探针定量分析的标准样品。经过测量和标定,这些单晶标样符合中华人民共和国国家标准GB 4930-85(电子探针显微分析标准样品通用技术条件)的规定。含有稀土元素的标样如NAB和YAP能发出绿色荧光,是电子显微术中理想的阴极发光材料。     

Balancing kinetic and thermodynamic control: the mechanism of carbocation cyclization by squalene cyclase

Molecular dynamics simulations with a combined quantum mechanical and molecular mechanical (QM/MM) potential have been carried out to investigate the squalene-to-hopene carbocation cyclization mechanism in squalene-hopene cyclase (SHC). The present study is based on free energy simulations by constructing the free energy surface for the cyclization steps along the reaction pathway. The picture that emerges for the carbocation cyclization cascade is a delicate balance of thermodynamic and kinetic control that ultimately favors the formation of the final hopanoids carbon skeleton. A key finding is that the five- to six-membered ring expansion process is not a viable reaction pathway for either C- or D-ring formation in the cyclization reaction. The only significant intermediate is the A/B-bicyclic cyclohexyl cation (III), from which two asynchronous concerted reaction pathways lead to, respectively, the 6,6,6,5-tetracyclic carbon skeleton and the 6,6,6,6,5-pentacyclic hopanoids. Experimentally, these two products are observed to have 1% and 99% yields, respectively, in the wild-type enzyme. We conclude that the product distribution in the wild-type enzyme is dictated by kinetic control of these two reaction pathways.     

高效液相色谱检测Zn（Ⅱ）、Cd（Ⅱ）、Co（Ⅱ）、Pb（Ⅱ）、Ni（Ⅱ）、Cu（Ⅱ）、Hg（Ⅱ）

用双-(2-羟乙基)二硫代甲酸铵(HEDC)在反相液相色谱中作检测某些金属离子的衍生化试剂，HEDC的金属螯合物微溶于水，可直接水样注射于C18柱中进行检测，范围为0．006～10mg／L相对偏差1％～2％，检测波长254nm，金属汞的整合物在HPLC分析前进行浓缩富集检测限可低至0．06～25μg／L，相对偏差小于2％。     

（η^2—C60）[Pt（PPh3）2]8的合成与表征

C60是高度共轭的宠状结构碳素体．分子结构中六元环间的共价碳碳双键是富电子区，其反应性能与烯键类似，以碳碳双键与中心金属形成η2配位化合物．富勒烯η2配合物的合成及性能研究是当前研究热点之一[1~7]．本文在（η2-C60）［Pt（PPh3）2］n（n=1～6）系列研究[7]的基础上制备了（η2－C60）［Pt（PPh3）2］8，并用元素分析、红外光谱和光电子能谱进行鉴定和表征．1实验部分四（三苯基膦）合铂Pt（PPh3）4按文献[8]方法制备；C60纯度为99％；其余试剂均为分析纯．元素分析在ERLA－1106型元素分析仪上进行；光电子能谱在VGESCA…